High temperature high pressure apparatus



June 21,

1960 R. H. WENTORF, JR

HIGH TEMPERATURE HIGH PRESSURE APPARATUS Filed Sept. 30, 1955 [r7 venton- Rob ert Wen oPfl/z',

- His Attorney subjected to high temperature and high .tions.

United States Patent HIGH TEMPERATURE HIGH PRESSURE APPARATUS Robert H. Wentorf, Jr., Schenectady, N.Y., assignor to General Electric Company, a corporation of New York Filed Sept. so, 1955, seam. 537,630

4 Claims. cits-16.5

My invention relates to high temperature high pres- :sure apparatus and specifically to such apparatus in which high temperatures and high pressures are maintained for prolonged periods of time.

In a copending application of Francis P. Bundy, Serial No. 488,042, filed February 14, 1955 and assigned to the same assignee as the present application, an apparatus is described to effect and control reactions occurring :at temperatures of the order of several thousand defgrees centigrade and pressures of the order of 20,000 :to 40,000 atmospheres for long time intervals. Such apparatus comprises a reaction vessel which is positioned between a pair of opposed, recessed dies to provide a :specimen chamber to be subjected to temperatures and pressures of the order mentioned.

A high temperature high pressure apparatus which provides a reaction vessel of increased size is desirable to accommodatelarger amounts of materials to be heated and pressed. In previous devices, reaction vessel size waslimited by thickness of the surrounding insulating and pressure resisting gasket. Such a gasket could be increased in size to enlarge the vessel but application of high pressure caused the gasket to extrude laterally from between opposed members with attendant loss of pressure in the reaction vessel. The invention of the presentapplication provides an apparatus which eliminates the previous gasket assembly and produces an in crease in reaction vessel size.

Accordingly, it is anobject of the invention to provide a new and improved high temperature high pressure apparatus.

.It is another object of the invention to provide an improved high temperature high pressure apparatus which increases the size of the reaction vessel.

It is a further object of the invention to provide an improved high temperature high pressure apparatus which eifectsand controls reactions at temperatures of over one thousand degrees centigrade and pr'essures of overi'4'0,000

atmospheres.

In carryingout my invention in one form, a r'eacsulating members between a pair of opposed, recessed dies to provide an enlarged specimen chamber which is pressure condi- These and various other objects, features, and advan- Fig. 1 is a front elevational view of a hydraulic press with a high temperature high pressure apparatus which embodies my invention; and

Fig. 2 is an enlarged sectional view of the high temperature high pressure apparatus which is shown in Fig. 1.

In Fig. 1 of the drawing, a hydraulic press comprises a base with a press bed 11 on which is mounted a 2 plurality of vertical shafts 12 to support a carriage 13. A ram 14 is mounted on the undersurface of carriage 13 to be actuated by an associated hydraulic piston 15 while a platen 16 is positioned centrally on press bed 11 in axial alignment with ram 14. Both ram 14 and platen 16 are recessed to partially position members17 therein, each of which comprises a central die 18 with surround ing binding rings 19. -An annular conducting ring'20 with a connector 21 is positioned around the periphery of each outer binding ring to supply electric current from a source of power (not shown) through rings19 and dies 18 to a high temperature high pressure reaction vessel which is described below. A layer of electrical insulation 22 is preferably provided between at least one member 17 and its associated platen 16 to prevent conduction of electric current through the press. If it is desired, conducting rings 20 can be connected to ram 14 and platen 16 to reduce the length of members 17.

As is best shown inFig. 2, the opposed or outer faces of dies 18 are recessed to provide a frusto-conical cavity 23 with an electrical and thermal insulating frusto-conical gasket 24 in contact therewith. Pressure resisting frusto-conical members 25 are positioned concentrically with and adjacent insulating gaskets 24 within cavity 23 of each die, and are positioned to project from the cavities 23 to provide outer abutting faces. The outer faces of opposed pressure resisting members 25 have an annular gasket or layer of electrical insulation 26 therebetween to prevent short-circuiting of the current path. Pressure resisting members 25 define a central aperture 27 which extends between opposed dies. While an electrically conductive object or specimen can be placed in aperture 27 to be subjected to hightemperature high pressure conditions, I prefer to employ a reaction vessel 28 within aperture 27 which vessel isin electrical contact with dies 18. Vessel 28 comprises a pairof spaced conductive discs 29 with'a hollow conductive tube 30 t-herebetween adapted to contain a specimen 31 to be subjected to high temperature high pressure conditions. A- hollow cylinder 32 of electrically insulating material is positioned around and engaging tube 30' between and in contact with discs 29 to complete the assembly of reaction vessel 28. If it is desired, reaction vessel 28'may be in the form of a hollow casing whichis in electrical contact with dies 18. A cap 33 is positionedbetwe'en each die 18 and its associated disc 29 to provide a thermal insulating core 34 with a surrounding outer conductive rim 35 in electrical contact with the die. Examples of suitable materials from which members 23, cylinder "32 and cores 34 can be made are pyrophylite and catlinite.' j

In the operation of the high temperaturehigh pressure apparatusshown in Figs. 1 and2, each member 17 with associated conducting ring'.18 and connector 19 1s positioned partially within the recess of'it's' associated ram 14 and platen 16 in the press. Specimen 31, which is to be subjected to a high temperature high pressure environment, is placed in tube 30 within cylinder 32-between discs 29 to complete reaction vessel 28. After a cap 33 is provided at each end of vessel 28, pressurefresisting members 25 are placed around'the vessel and cap 33 to enclose the structure. A layer of electrical insulation 26 is positioned between opposed or abutting faces of members 25 to prevent conduction of electrical current therebetween. Electrical and thermal insulating members 24 surround members 25 to provide an outer insulating layer. The assembly is then positioned within opposed frusto-conical cavities 23 of dies 18 to complete the high temperature high pressure apparatus. Pressure which is supplied by piston 15 through its associated ram 14 and member 17 is applied to specimen 31 by opposed dies 18. At the same time, electric current 15 supplied from one electrical connector, such as, upper connector 21 to upper conducting ring 20, binding rings 19, dies '18," rim 3'5; and" disc 29 to generate nearin'tnbe 30 of vessel 28. The current path continues through lower disc, 35, dies 1}}, binding rings 19, con; ducting ZDQaiid connector zlf'tof the," trical'spurce. prepares in games of room-armored sand empretureshigher than ,1,000' C. hav 'b', n maintained in such apparatus for periods of hours; Ifit'is desired, reaction vessel 28 nia y also beisubjected t igh ie srirssa s e-T" be apparent to those skilled in the art, the ob e ts a m venti'snare a t in t u e of a reaction vessel which is positioned within apairof'inner pressure resisting members and outer electrical andth'erinsul ting members betweena pair 'of opposed, "recessed dies to provide an enlarged specimen chamber to be subjected to high temperature and high pressure cg n i ynl H While otherrnodifications of this invention and variations of apparatus have not been described, the invention is intended to include all such as 'may be em braced within the following claims.

-What I claim asnew and-desire tosecure by Letters Raw 9 th U i d a e 1 1. High temperature high-pressure apparatus comprisinga pair of opposed dies, means forfex erting pressure against hat leastone of said dies, at layer ofinsulation between one of said dies and its associated pressure means, ,an electrical connection to each of said dies, th e opposed outer faces of said dies being recessed to provide a cavity therein, an electrical and thermal insulat' ing gasket 'in contact with the wall of each of said cavities, a pressure resisting member concentrically with and adjacent each said insulating gasket and projecting from said cavities to provide abutting faces, said pres sure resisting members forming a central aperture between said dies adapted to contain an object to'be sub jected to high temperature high pressure conditions, and La layerof insulation between adjacent abutting faces of ,said pressure resisting members.

High temperature high pressure apparatus comprisingfa pair of, opposed members, means for exerting pressure against at least one of said members, a layer ofinsulation between ,one'of said members and its as sociated lpressnre rncausgfinfelectrical connection to each of said members, each member comprising a die, at'least one bindi ng ringlaround said die, was opposed faces of said dies being-recessed to provide a conical cavity there in, electrical and thermal insulating frusto-conical gasket incontact with the wall ofeach of said cavities,

-;a pressure resisting frusto conicaYmember concentric with and adjacent said insulating gasket, v nd projecting from said cavities to provide abutting faces, said, pressure resistingmentbersforming a central aperture betweensaidfdies adapted to contain ,a"sp,ec'i'men to be bj ected to high temperature high pressure" conditions, ,and; a layeryof insulation between adjacent abutting faces o ;said pressure resisting members.

3. High temperature high pressure apparatuscomprising a pair of opposed members, means for exerting'pres- ,sure against at least one of said members, alayer of insulation between one of said members and its associated pressuremeans, an electrical 7 connection to each of said 4 1 members, each member comprising a die, at least one binding ring around said die, each-of the opposed outer faces of said dies being recessed to provide a frusto conical cavity, an electrical and thermal insulating fmsto conical gasket for each cavity and in contact with the wall of its associated cavities, a pressure resisting frustoconical member concentric with and adjacent each of said insulating gaskets, and projecting from said cavities to provide abutting faces, said pressure resisting members forming a central aperture, 2; reaction vessel located within said aperture adaptedto contain a specimen to be subjected to high temperature high pressure conditions, said vessel being in electrical contact with said dies, and a layer ofinsulation'between adjacent abutting faces of said pressure resisting members.

4. High temperature high pressure apparatus comprising a pair of opposed members, means for exerting pressure againstat least one of said members, a layer of insiilatioii between one of said rnernbersand its associated pressure means, an electrical connectionto each ofsaid members, eachmember comprising "ajdie, at least one binding ring around said die, e'ajchof'the opposed outer races of said dies being recessedto provide 'a' frusto-conicaleav'ity, anelect'rical and thermal insulating frusto-crpnical fgasket ior'e'ach cavity and in contaetfwithfthe'wall ofeacli of said cavities, a pressure resistin'g'frusto-jconical member positioned concentrically within and adjacent said insulating gaskets, and projecting f from said cavities to' provide abutting 'faces, a layer or insulationjfbetween adjacent abutting faces'of said'pr'es sure resisting members, said pressure resistinginembers forming a central aperture, a reaction vessellocatedj'within said aperture, said vessel comprising a pair of spaced" c'onductiv e'discs, a hollow conductive tube"adapted to'conta'in' aspecimen to be' subjected to high temperature high pressure'conditions positioned between said ,discs,""an electrical and thermal insulating cylinder around, and engaging said tube and said discsja cap adjacent the end of eacho'f said discs, said'cap comprisinga heat insulating core, and an outer conductive riin'surrounding said core, said rim bein electricalcohtact with its associated die;

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